Granted Patent B2

US 12,384,717 · App. 17/642,432 · Granted Aug 12, 2025

Inventors: David Eugene Baker (Bath, NY); Albert Joseph Fahey (Corning, NY); Qiang Fu (Painted Post, NY); Yuhui Jin (Painted Post, NY); Wei Sun (Painted Post, NY); Ljerka Ukrainczyk (Ithaca, NY); Shelby Kerin Wilson (Corning, NY)

Assignee: CORNING INCORPORATED

C03C21/002

Abstract

Claims (22)

1. A method for regenerating a salt bath composition, the method comprising:

heating the salt bath composition to an ion exchange temperature to form a molten salt bath;

contacting at least a portion of an ion-exchangeable article comprising lithium oxide with the molten salt bath, whereby lithium cations diffuse from the ion-exchangeable article and into the molten salt bath;

adding a first phosphate salt to the molten salt bath, whereby a lithium phosphate salt comprising at least a portion of the lithium cations is formed and precipitates from the molten salt bath; and

adding a multivalent salt comprising a multivalent metal cation to the molten salt bath, whereby a second phosphate salt comprising the multivalent metal cation is formed and precipitates from the molten salt bath.

2. The method of claim 1 , wherein the salt bath composition comprises:

from 40 wt. % to 95 wt. % potassium nitrate based on the total weight of the salt bath composition;

from 5 wt. % to 60 wt. % sodium nitrate based on the total weight of the salt bath composition; and

from 0.1 wt. % to 1 wt. % lithium nitrate based on the total weight of the salt bath composition.

3. The method of claim 1 , wherein the salt bath composition comprises from 0.1 wt. % to 1 wt. % silicic acid based on the total weight of the salt bath composition.

4. The method of claim 1 , wherein the ion exchange temperature is greater than or equal to 450° C.

5. The method of claim 1 , wherein the ion-exchangeable article comprises from 2 mol. % to 25 mol. % lithium oxide.

6. The method of claim 1 , wherein the ion-exchangeable substrate comprises glass or glass-ceramic.

7. The method of claim 1 , wherein the first phosphate salt is selected from the group consisting of trisodium phosphate, tripotassium phosphate, disodium phosphate, dipotassium phosphate, sodium triphosphate, potassium triphosphate, disodium diphosphate, tetrasodium pyrophosphate, potassium pyrophosphate, sodium trimetaphosphate, potassium trimetaphosphate, and combinations thereof.

8. The method of claim 1 , wherein a concentration of the lithium cations in the molten salt bath is greater than or equal to a concentration of the first phosphate salt.

9. The method of claim 1 , wherein the precipitation of the lithium phosphate salt reduces a concentration of the lithium cations in the molten salt bath by greater than or equal to 0.03 wt. % based on the total weight of the molten salt bath.

10. The method of claim 1 , wherein the lithium phosphate salt comprises at least one of insoluble trilithium phosphate, insoluble dilithium sodium phosphate, or insoluble lithium disodium phosphate.

11. The method of claim 1 , wherein the multivalent metal cation is selected from the group consisting of magnesium, calcium, aluminum, strontium, barium, iron, and combinations thereof.

12. The method of claim 1 , wherein the multivalent salt comprises calcium nitrate.

13. The method of claim 1 , wherein the precipitation of the second phosphate salt reduces a total concentration of phosphate salts in the molten salt bath to less than 0.01 wt. % based on the total weight of the molten salt bath.

14. The method of claim 1 , further comprising removing the ion-exchangeable article from contact with the molten salt bath, wherein the ion-exchangeable article is removed before adding the first phosphate salt and adding the multivalent salt.

15. The method of claim 1 , wherein the multivalent salt is added to the molten salt bath in an amount from 0.01 wt. % to 0.5 wt. %.

Assignments (1)

Continuity (2)

References Cited (19)